The preparation of salts containing the tetrathioperrhenate anion was first reported in 1931. See, Feit, W., Angew. Chem. 1931, 44, p. 65). Other preparative techniques have subsequently been reported. See, for example, Muller, et al., Chem. Ber. 1970, 103, p. 2961, which calls for bubbling hydrogen sulfide through a dilute solution of ReO.sub.4 -- in aqueous ammonium hydroxide, and Muller, et al., Chimia 1986, 40, p. 50, which calls for adding Re.sub.2 O.sub.7 to a methanol polysulfide solution which is heated and allowed to stand for one to two days. None of these reported procedures are especially suitable for the preparation of significant quantities of tetrathioperrhenate salts, however, because of the poor yields obtained, the length of time that is required in carrying the reaction, or indeed the complexity of preparation of the reagents employed in the synthetic procedure.